®
Comparison of Two-Dimensional Gas Chromatography and Tandem Mass Spectrometry for Pesticide
Analysis of Herbal Teas
Michelle Misselwitz, Julie Kowalski, Jack Cochran
®
Herbal Teas – Ancient Medicine Nettle - Remedies for an assortment of ailments including anemia, high blood
pressure, rheumatism, arthritis, coughs and colds, congestion, urinary tract infections, and kidney and bladder problems.
Chamomile Tea - Soothes the stomach and relieves bloating and indigestion. Calms the mind and helps people relax and deal better with their stresses.
Ginger Tea - Stimulates and soothes the digestive system. Ginger has been known to aid people experiencing nausea.
Peppermint Tea - Helps you digest foods better and also reduces flatulence and digestive issues. Eases nausea and vomiting, especially if you suffer motion sickness.
Hibiscus Flower Tea (Sorrel) - Lower blood pressure, reduce high cholesterol and strengthen the immune system (it’s rich in Vitamin C.
Lemon Balm Tea - Effective tonic to calm nerves and anxiety.
Green Tea - the ‘wonder herb’ lowers cancer risk and contains potent antioxidants. Green tea also lowers blood pressure, prevents and fights tooth decay and dental
issues, and inhibits different viruses from causing illnesses.
®
Organochlorine
Organonitrogen
Pyrethroid
Triazole
Fungicide
Insecticide Herbicide
Synergist Acaricide
Plant Growth Regulator
Organophosphorus
®
Herbal Teas Targeted Pesticide Analysis
Wild Berry Zinger Ingredients: Hibiscus, rosehips, roasted chicory, orange peel,
blackberry leaves, natural flavors of black raspberries, strawberries, blueberries, red raspberries, cranberries and
cherries
Pau d’Arco A Traditional South American Herbal Tea
Contains: Pau d’Arco bark
Red Tea – Cinnamon Orange Ingredients: Rooibos, cinnamon, orange peel, natural cinnamon
and orange flavors
Everyday Detox Ingredients: roasted chicory root, dandelion root, schisandra fruit, lycium fruit, lycium fruit, licorice root, ginger rhizome, star anise
fruit, kukicha twig (85% Certified Organic Ingredients)
®
QuEChERS Performance Standards Mix A
Acephate Diazinon
Dichlorvos Dimethoate Malathion
Methamidophos Mevinphos Omethoate Chlorpyrifos Coumaphos
Fenthion Pirimiphos methyl Azinphos methyl
Mix C Carbaryl
Methiocarb Iprodione Metalaxyl Vinclozolin
Captan Myclobutanil Deltamethrin
Bifenthrin cis-Permethrin
Imazalil trans-Permethrin
Cyprodinil Fenpropathrin
Folpet Thiabendazole
Fenhexamid
Mix B Chlorothalonil
4,4'-DDT Dichlofluanid
Dicofol Endrin
o-Phenylphenol Propargite
Endosulfan sulfate Phosalone
gamma-BHC
Red = Tea leaves Purple = Hibiscus Teal = Citrus Italics = Chicory Blue = Ginger
®
QuEChERS – Extraction 1 g ground tea
+ 10 mL H2O
Soak 30 min
+ 10 mL Acetonitrile
+ QuEChERS GC/MS Internal Standard
+ Pesticide spike mix
Vortex 30 min
Add EN Buffer Salts 4 g magnesium sulfate
1 g sodium chloride 1 g trisodium citrate dihydrate 0.5 g disodium hydrogencitrate
sesquihydrate
Shake 1 min
Centrifuge 5 min
®
500 pg ISTD
Complex Samples
®
% Recoveries of Fortified Tea at 1000 ng/g (100 pg on-column) quantified using GC-MS
Pau d'Arco Tea Zinger Tea Red Tea Detox Tea
Acephate ND ND ND ND
o-Phenylphenol 86 84 87 89
Omethoate 120 ND ND ND Diazinone 93 79 91 94 Chlorothalonil 62 72 82 79
Vinclozoline 88 81 87 87 Carbaryl 94 80 91 95
Metalaxyl 84 84 86 91
Methiocarb 91 79 92 96
Malathion 100 80 89 93
Fenthion 87 81 89 89
Chlorpyrifos 88 76 90 88 Cyprodinil 80 59 82 80
Thiabendazole 44 54 48 ND Captan 97 86 100 120
Imazalil 81 82 84 100
Endosulfan sulfate 110 76 81 93 Propargite 94 73 101 ND
Iprodione 89 76 94 100 Bifenthrin 86 68 83 87
Fenpropathrin 100 76 90 89 cis-Permethrin 87 67 82 ND
Deltamethrin 92 71 95 110
®
Cartridge SPE Cleanup
1 mL extract
Combo SPE Cartridge, 6mL/500mg Carboprep®,
90/500mg PSA
Add MgSO4 to tube
Elute 15mL acetone: toluene (3:1)
®
Cartridge SPE Cleanup
1 mL extract
MgSO4
500 mg GCB
500 mg PSA
Elute 15 mL 3:1 Acetone:Toluene
Concentrate to1 mL
®
Dispersive SPE (dSPE cleanup)
1 mL extract
Shake 2 min
Centrifuge 5 min
Q252 Q213
Guide to Sorbents
Removes Sugars and fatty acids Primary secondary amine (PSA)
Sorbent
Octadecyl (C18) Lipids
Pigments and sterols Graphitized carbon black (GCB)
dSPE Cleanup
150 mg MgSO4, 50 mg PSA, 50 mg C18, 7.5 mg GCB
®
GCxGC vs GC-MS/MS
Chromatographic Separation Resolution!
Full Spectral Information!
Mass Spectrometer Separation Selectivity! Sensitivity!
®
GCxGC Schematic
Modulator
1st Dimension 2nd Dimension
From Injector
To Detector
Focuses effluent from primary column (cold jet) and “injects” this effluent
(hot jet) to secondary column
Fast detector to record 50-500 ms wide peaks
Orthogonal GC column stationary phases means two independent separation mechanisms
®
Modulator
1st Column 2nd
Column
Inlet
Detector
Linear Chromatogram
2n
d C
olu
mn
Fundamentals of GCxGC
Surface Plot Contour Plot
®
+ +
+
+
+ +
time m/z
110
245 89
+
+
+
+ +
+ +
+
+ +
+
+
+
+
+
Q1
+ + +
+
+
+
+ +
+ +
m/z
99
133
68
+ + +
+
+
+
+
+ + +
Q3 Q2
Fragment Ions
+
Triple Quadrupole
®
MSn for Signal-to-Noise Improvement
0 1 2 3 4 5 6
Stages of Analysis
Inte
nsi
ty
Signal
Noise
S/N
Sensitivity
®
GC X GC Conditions Injection
Temp: 250°C Injection:1 µL fast, splitless (1.0 min) Liner: Sky Single Taper
Column
Rxi Guard 1.0 m x 0.25 mm Rxi-5ms 30 m x 0.25 mm x 0.25 µm Rtx-200 1.0 m x 0.25 mm x 0.25 µm Column connector: SGE SilTite µ-Union
Conditions Oven: 70°C (1 min), 8°C/min to 330°C (6.5 min) Secondary Oven Offset: + 5°C Carrier: He, constant flow 1.4 mL/min Modulator Temperature Offset: 20°C Modulation Time: 2 sec
LECO Pegasus®
TOFMS Conditions
Transfer Line Temperature: 320°C
Source Temperature: 225°C
Electron Ionization: 70 eV
Stored Mass Range: 45 to 550 u
Acquisition Rate: 100 spectra/sec
GCxGC-TOFMS Conditions
®
GC-MS/MS Conditions GC Conditions
Injection
Temp: 250°C Injection:1 µL fast, splitless (1.0 min) Liner: Sky Single Taper with wool
Column
Rxi-5ms 30 m x 0.25 mm x 0.25 µm
Conditions Oven: 70°C (1 min), 8.7°C/min to 330°C (5 min) Carrier: He, constant flow 1.4 mL/min
Thermo TSQ 8000 GC-MS/MS
Transfer Line Temperature: 280°C
Source Temperature: 250°C
Electron Ionization: 70 eV
Acquisition: SRM, 3 per analyte
Total Scan Time: 0.150 sec
®
Liner choice : wool or no wool?
Wool No Wool
Better response for thermal labile pesticides
Better response for more active pesticides
Controlled sample introduction
Protects GC column from non-volatile residue
®
Complex Samples
After 28 tea injections!
Use wool in your splitless liner to protect
your GC column from non-volatile dirt
®
Methamidophos
Dichlorvos
No retention
gap
1 m retention
gap
No Wool - Retention Gap - better solvent focusing
®
Pau d’Arco A Traditional South American Herbal Tea
Contains: Pau d’Arco bark
1.0
m x
0.2
5 m
m x
0.2
5 µ
m R
tx-2
00
1.0 m x 0.25 mm Rxi Guard + 30 m x 0.25 mm x 0.25 µm Rxi-5ms
®
RT: 0.0 - 28.9
0 5 10 15 20 25
Time (min)
0
50
100
0
50
100
0
50
100
0
50
100
0
50
100
Relative
Abunda
nce 0
50
100
0
50
100
0
50
10011.2
11.0
12.2
12.3
16.3
16.416.2
17.1
17.017.2
17.7
17.9
22.8
22.922.6
25.0
25.2
25.3
16.915.8
17.7 21.7
22.418.412.228.611.18.0
NL: 6.94E4
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [42.095-42.105] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 1.84E6
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [115.095-115.105] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 3.04E4
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [132.995-133.005] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 5.09E4
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [123.995-124.005] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 2.56E5
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [153.095-153.105] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 2.59E4
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [244.995-245.005] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 1.30E5
m/z= 42.10-286.00 F: + c EI SRM ms2 [email protected] [168.095-168.105] MS Pau_d_Arco_Spike_10ppbDUP_inj7
NL: 1.67E7
TIC MS Pau_d_Arco_Spike_10ppbDUP_inj7
Pau d’Arco A Traditional South American Herbal Tea
Contains: Pau d’Arco bark
30 m x 0.25 mm x 0.25 µm Rxi-5ms
®
% Recoveries of Spiked Pesticides in Pau d’Arco Tea (n=2)
Pesticide 1000 ng/g 100 ng/g
GC-MS/MS GCxGC-TOFMS GC-MS/MS GCxGC-TOFMS
Acephate 100 90 78 65
o-Phenylphenol 101 87 77 100
Omethoate 88 96 76 58
Diazinon 101 99 94 99
Chlorothalonil 56 71 65 58
Vinclozolin 96 90 92 84
Carbaryl 61 98 80 65
Metalaxyl 99 100 83 97
Methiocarb 72 100 94 73
Malathion 102 100 86 91
Fenthion 98 100 88 90
Chlorpyrifos 94 91 81 87
Cyprodinil 85 86 75 66
Thiabendazole 68 58 66 39
Captan 73 110 90 72
Imazalil 101 80 78 80
Endosulfan sulfate 88 95 87 82
Propargite 89 99 84 70
Iprodione 92 120 92 27
Bifenthrin 92 91 83 77
Fenpropathrin 96 96 93 85
cis-Permethrin 93 100 87 78
Deltamethrin 85 94 94 45
®
o-Phenylphenol
GCxGC - Spectral Deconvolution
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 135
152
77
63
107
121 169 434 285 399 357 231
Caliper - sample "Pau d'Arco Tea extract:1", 786 , 0.790 sec , sec to 786 , 0.790 sec , sec - 150 , 0.000 sec , sec to 150 , 0.000 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 65
169
141
115
87
47 434 285 356
Peak True - sample "Pau d'Arco Tea extract:1", peak 292, at 786 , 0.790 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 170
115 141
63 89 39
155
Library Hit - similarity 948, "o-Phenylphenol"
Caliper
Peak True
Library Hit
®
0.72786
0.74786
0.76786
0.78786
0.8786
0.82786
0
1000
2000
3000
4000
5000
6000
7000
1st Time (s)2nd Time (s)
170 135
GCxGC - Spectral Deconvolution
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 135
152
77
63
107
121 169 434 285 399 357 231
Caliper - sample "Pau d'Arco Tea extract:1", 786 , 0.790 sec , sec to 786 , 0.790 sec , sec - 150 , 0.000 sec , sec to 150 , 0.000 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 65
169
141
115
105 87
434 285 356
Peak True - sample "Pau d'Arco Tea extract:1", peak 292, at 786 , 0.790 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 170
115
141
63
89 74
102 155
Reference Spectrum - Calibration "QuEChERS Perf AB 500", Analyte "o-Phenylphenol"
Caliper
Peak True
Reference Spectrum
o-P
hen
ylp
hen
ol
un
kno
wn
®
MS/MS Selectivity
141 > 115.1 m/z 169.7 > 115.1 m/z 169.7 > 141.3 m/z
(mainlib) o-Hydroxybiphenyl
20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 1800
50
100
27
39 51
52 5558
62
63
65 7077 87
89
91 98102
115
126 131
141
151 155
170
OH
o-phenylphenol
®
Pau d’Arco
A Traditional South American Herbal Tea Contains: Pau d’Arco bark
Average % Recovery for ALL target pesticides
Spike GC-MS/MS GCxGC-TOFMS
1000 ng/g 93% (± 15) 92% (± 14)
100 ng/g 87% (± 12) 81% (± 17)
10 ng/g 84% (± 24) NA
GCxGC-TOFMS Thiabendazole (130) Fenpropathrin (43)
Incurred Pesticides (ng/g):
GC-MS/MS Thiabendazole (16)
Imazalil (13)
®
Wild Berry Zinger Ingredients: Hibiscus, rosehips, roasted chicory, orange peel, blackberry leaves, natural flavors…
®
% Recoveries of Spiked Pesticides in Wild Berry Zinger Tea
Pesticide 1000 ng/g 100 ng/g
GC-MS/MS GCxGC-TOFMS GC-MS/MS GCxGC-TOFMS
Acephate 76 88 88 81
o-Phenylphenol 86 92 113 95
Omethoate 81 78 101 88
Diazinon 85 93 86 95
Chlorothalonil 72 79 74 100
Vinclozolin 84 99 89 91
Carbaryl 98 94 89 91
Metalaxyl 86 96 84 90
Methiocarb 84 90 85 89
Malathion 91 95 96 94
Fenthion 84 88 85 98
Chlorpyrifos 84 93 84 88
Cyprodinil 65 71 66 73
Thiabendazole 65 62 86 77
Captan 86 99 102 180
Imazalil 86 91 102 91
Endosulfan sulfate 86 95 87 100
Propargite 85 96 84 110
Iprodione 88 99 85 74
Bifenthrin 76 86 77 82
Fenpropathrin 85 93 97 93
cis-Permethrin 78 88 78 70
Deltamethrin 83 88 74 78
®
Ingredients: Hibiscus, rosehips, roasted chicory, orange peel, blackberry leaves, natural flavors…
Wild Berry Zinger
Average % Recovery for ALL target pesticides
Spike GC-MS/MS GCxGC-TOFMS
1000 ng/g 79% (± 10) 90% (± 11)
100 ng/g 83% (± 12) 94% (± 33)
10 ng/g 88% (± 19) NA
GCxGC-TOFMS Carbaryl (10)
Chlorpyrifos (16) Imazalil (727)
Thiabendazole (429) o-Phenylphenol (22)
Incurred Pesticides (ng/g):
GC-MS/MS Carbaryl (23)
Chlorpyrifos (18) Imazalil (470)
Thiabendazole (240) Fenhexamid (2)
4’4-DDT (1)
®
Red Tea – Cinnamon Orange Ingredients: Rooibos, cinnamon, orange
peel, natural cinnamon and orange flavors
®
% Recoveries of Spiked Pesticides in Red Tea
Pesticide 1000 ng/g 100 ng/g
GC-MS/MS GCxGC-TOFMS GC-MS/MS GCxGC-TOFMS
Acephate 69 110 74 80
o-Phenylphenol 86 98 83 96
Omethoate 58 120 66 100
Diazinon 84 99 94 88
Chlorothalonil 69 110 71 71
Vinclozolin 85 100 88 83
Carbaryl 83 110 82 85
Metalaxyl 85 110 84 87
Methiocarb 83 120 90 102
Malathion 85 110 93 77
Fenthion 83 110 84 91
Chlorpyrifos 81 100 88 90
Cyprodinil 75 97 78 79
Thiabendazole 52 87 51 75
Captan 89 140 76 160
Imazalil 73 120 76 88
Endosulfan sulfate 80 120 80 84
Propargite 78 110 89 92
Iprodione 82 120 89 92
Bifenthrin 74 98 78 85
Fenpropathrin 80 110 74 76
cis-Permethrin 74 99 76 92
Deltamethrin 77 120 93 120
®
Rooibos, cinnamon, orange peel, natural cinnamon and orange flavors
Spike GC-MS/MS GCxGC-TOFMS
1000 ng/g 83% (± 8) 110% (± 13)
100 ng/g 87% (± 12) 91% (± 14)*
10 ng/g 90% (± 15) NA
GCxGC-TOFMS o-Phenylphenol (25)
Incurred Pesticides (ng/g):
GC-MS/MS o-Phenylphenol (20)
Endosulfan sulfate (2) Iprodione (2) Imazalil (2)
Thiabendazole (8)
Red Tea – Cinnamon Orange
®
Red Tea – Cinnamon Orange Incurred Imazalil
2 ng/g = 0.2 pg on-column
Quant peak 215 > 173 m/z
Confirming Ion Ratio ± 20% 3 SRM transitions
®
Everyday Detox Ingredients: roasted chicory root, dandelion root, schisandra fruit, lycium fruit, licorice root, ginger
rhizome, star anise fruit, kukicha twig
®
GCxGC Resolution
Acephate m/z 136
®
Acephate MS/MS Selectivity
Quant peak 136 > 42.1 m/z
100 pg on-column
10 pg on-column
Corruption of peak from
interferences
Confirming ions 94 > 64 m/z
136 > 94 m/z
®
Acephate has a “skinny” mass spectrum. There is not a lot of high abundance, high m/z values for more “selective” fragmentation
®
% Recoveries of Spiked Pesticides in Everyday Detox Tea
Pesticide 1000 ng/g 100 ng/g
GC-MS/MS GCxGC-TOFMS GC-MS/MS GCxGC-TOFMS
Acephate 75 88 81 89
o-Phenylphenol 85 88 81 100
Omethoate 66 85 95 93
Diazinon 87 88 78 96
Chlorothalonil 73 74 71 99
Vinclozolin 84 93 83 110
Carbaryl 86 97 74 100
Metalaxyl 85 100 76 88
Methiocarb 86 96 78 120
Malathion 86 98 75 67
Fenthion 87 98 81 100
Chlorpyrifos 85 88 84 110
Cyprodinil 75 83 69 81
Thiabendazole 62 75 37 86
Captan 82 100 82 100
Imazalil 84 75 63 72
Endosulfan sulfate 87 99 77 100
Propargite 89 90 83 83
Iprodione 91 90 81 100
Bifenthrin 81 85 75 84
Fenpropathrin 88 90 83 100
cis-Permethrin 80 87 67 97
Deltamethrin 86 90 89 93
®
roasted chicory root, dandelion root, schisandra fruit, lycium fruit, licorice root, ginger rhizome, star anise
fruit, kukicha twig
Spike GC-MS/MS GCxGC-TOFMS
1000 ng/g 85% (± 28) 89% (± 10)
100 ng/g 79% (± 13) 97% (± 24)
10 ng/g 87% (± 19) NA
GCxGC-TOFMS None Found
Incurred Pesticides (ng/g):
GC-MS/MS gamma-BHC (1) Methiocarb (6)
Everyday Detox
®
GCxGC TOFMS Benefits/Drawbacks
+ Non- target screening possible
+ High identification confidence: 2 retention times and full mass spectrum
+ Interferences: simple reprocessing of data with different quant ion
- More difficult GCxGC hardware setup and method development
- Higher detection limits
- Large data files and slower data processing
®
GC-MS/MS Benefits / Drawbacks
+ Lower Detection Limits – most compounds easily detected at 1 pg on-column
+ Faster data processing/smaller file sizes
+ Easier hardware setup
- Targeted screening only
- More difficult compound identification (management of ion ratios and allowable deviation)
- Less identification confidence: one retention time and limited mass spectral information
- Time consuming MS method development
®
Conclusions
• A QuEChERS extraction and dSPE cleanup of herbal teas resulted in good recoveries of target pesticides.
• Using GC-MS/MS allowed detection of target pesticides at 10 ng/g.
• Non-target screening of active ingredients is possible with GCxGC-TOFMS.
• Average percent recoveries were similar for both instrument platforms.
®
Non-Target Analysis
Maté Lemon Ingredients: Yerba maté, lemon myrtle, green tea
“Its stimulating effect evokes a cheerful mental lucidity”
Sceletium & Honeybush Tea Ingredients: Sceletium and african honeybush
“The cup that cheers”
elev8 Ingredients: Zembrin 25 mg, equivalent to 50 mg
Sceletium tortuosum above ground herb
®
Maté Lemon Ingredients: Yerba maté, lemon
myrtle, green tea
®
Peak Find, Spectral Deconvolution, Library Search
Set S/N, automatic deconvolution
®
Sort by Similarity for Qualitative Review
®
Maté Lemon Ingredients: Yerba maté, lemon
myrtle, green tea
1425 peaks S/N ≥ 100
®
Some names are easily recognized.
Qualitative Review
100 200 300 400 500
1000 67
194
Caliper - sample "Mate Lemon Tea extract:1", 1206 , 1.190 sec , sec to 1206 , 1.190 sec , sec - 400 , 0.000 sec , sec to 400 , 0.000 sec , sec
100 200 300 400 500
500
1000 67
194
Peak True - sample "Mate Lemon Tea extract:1", peak 931, at 1206 , 1.190 sec , sec
100 200 300 400 500
500
1000 194
109
55
Library Hit - similarity 941, "Caffeine"
Caffeine
®
Others may need further investigation.
Qualitative Review
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 78
51
122
106
94
Caliper - sample "Mate Lemon Tea extract:1", 610 , 1.420 sec , sec to 610 , 1.420 sec , sec - 400 , 0.000 sec , sec to 400 , 0.000 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 78
51
122
106
94 67
Peak True - sample "Mate Lemon Tea extract:1", peak 559, at 610 , 1.420 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 122
78
106
51
94 66
Library Hit - similarity 912, "Niacinamide"
Niacinamide is part of the vitamin
B group. It has anti-inflammatory,
anti-anxiety properties.
Be critical with NIST library matches. Is it real? More unique
spectrum with abundant high m/z
ions gives better confidence in match.
®
Recognizing chemical names can sometimes be difficult. Using the synonym list is helpful. “Pyridine, 2-chloro-6-(2-furanylmethoxy)-4-
(trichloromethyl)-” is also known as Pyroxyfur, a fungicide.
Qualitative Review
®
Qualitative Review
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
107 71
Caliper - sample "Mate Lemon Tea extract:1", 514 , 1.110 sec , sec to 514 , 1.110 sec , sec - 400 , 0.000 sec , sec to 400 , 0.000 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
107
Peak True - sample "Mate Lemon Tea extract:1", peak 462, at 514 , 1.110 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
Library Hit - similarity 910, "Pyroxyfur"
Pyroxyfur is a pyridine fungicide.
With less spectral information it is difficult to assign a positive match.
®
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
107 71
Caliper - sample "Mate Lemon Tea extract:1", 514 , 1.110 sec , sec to 514 , 1.110 sec , sec - 786 , 0.708 sec , sec to 786 , 0.708 sec , sec
45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125
200
400
600
800
1000 81
53
51 107 55
Peak True - sample "Mate Lemon Tea extract:1", peak 462, at 514 , 1.110 sec , sec
45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125
200
400
600
800
1000 81
53
51
Library Hit - similarity 910, "Pyridine, 2-chloro-6-(2-furanylmethoxy)-4-(trichloromethyl)-"
Peak True matches Library Hit at low m/z values
Peak True
Library Hit
®
Qualitative Review
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
107 71
Caliper - sample "Mate Lemon Tea extract:1", 514 , 1.110 sec , sec to 514 , 1.110 sec , sec - 400 , 0.000 sec , sec to 400 , 0.000 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
107
Peak True - sample "Mate Lemon Tea extract:1", peak 462, at 514 , 1.110 sec , sec
50 100 150 200 250 300 350 400 450 500 550
200
400
600
800
1000 81
53
Library Hit - similarity 910, "Pyroxyfur"
With less spectral information it is difficult to assign a positive match.
®
305 310 315 320 325 330 335 340 345 350
200
400
600
800
1000
Caliper - sample "Mate Lemon Tea extract:1", 514 , 1.110 sec , sec to 514 , 1.110 sec , sec - 786 , 0.708 sec , sec to 786 , 0.708 sec , sec
305 310 315 320 325 330 335 340 345 350
5
10
15
20
Peak True - sample "Mate Lemon Tea extract:1", peak 462, at 514 , 1.110 sec , sec
305 310 315 320 325 330 335 340 345 350
5
10
15
20
Library Hit - similarity 910, "Pyridine, 2-chloro-6-(2-furanylmethoxy)-4-(trichloromethyl)-"
No molecular weight ion in Peak True spectrum
Pyroxyfur MW = 325
Peak True
Library Hit
®
Flavonoids – polyphenolic compounds that may reduce
the risk of certain cancers.
Structured Chromatograms Sceletium & Honeybush
Tea
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Phytosterols – may help reduce blood cholesterol
levels.
Structured Chromatograms Sceletium & Honeybush
Tea
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β-Sitosterol
Stigmasterol Campesterol
Structured Chromatograms
Phytosterols Sceletium & Honeybush
Tea
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The South African Sceletium tortuosum herb has been extracted for the medicinally relevant mesembrine-type alkaloids.
Mesembranol Mesembrine Mesembrenol Mesembrenone
The mesebrine-type alkaloids have shown to elevate mood, reduce stress
and promote a sense of calm
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m/z 204, 218, 289
Mesembrine-type alkaloids elev8TM
“elevates mood, assists in coping with stress”
Sceletium and Honeybush Tea
“The Cup that Cheers”
The minor mesembrine alkaloid mesembranol was not detected in the tea sample, however many other beneficial compounds (phytosterols, flavonoids) that were present
in the tea were not in the tablet.